The synthesis and X-ray crystal structure determination of a novel metal-terphenyl derivative, namely DmpAuPPh(3) (1). is reported (Dmp = 2,6-dimesitylphenyl). Complex 1 is synthesized by the reaction of one equivalent of DmDLi with one equivalent of Ph3PAuCl in tetrahydrofuran at room temperature in 70% yield. The molecular structure of monomeric 1 features a two-coordinate gold atom with an essentially linear arrangement of the two ligands with an interligand angle of 174.21(8)degrees as well as a slightly tilted terphenyl moiety. (C) 2001 Elsevier Science B.V. All rights reserved.